• Korean Journal of Food Science and Technology
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• v.40 no.1
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• pp.8-14
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• 2008

This study was performed to establish analysis methods, and evaluated for grayanotoxin in domestic/foreign honey and wild honey. The molecular weight of grayanotoxins I, II and III, excluding grayanotoxin III that has been commercialized, were analyzed by LC-MS/MS. Then, the molecular structure of grayanotoxins I and II were analyzed by NMR. A total 111 samples (25 Korean honey, 21 Korean wild honey, 13 Korean honeycomb honey, 44 foreign honey, 8 foreign wild honey) were examined to determined whether or not each sample contained grayanotoxins I, II, and III. The honey samples were mixed with methanol and loaded into a tC18 cartridge, the filtrate was diluted with water, and the mixture was then analyzed by ESI triple-quadrupole LC-MS/MS. Grayanotoxins were only found in the foreign wild honey and were not detected in Korean honey, Korean honeycomb honey, or Korean wild honey. Three of the samples contained grayanotoxin I, II, and III, and one sample contained only grayanotoxins I and III. The lowest level for grayanotoxin I was 3.13 ${\pm}$ 0.00 mg/kg, and the highest level was 12.93 ${\pm}$ 0.01 mg/kg. The levels of grayanotoxin II were 0.84 ${\pm}$ 0.01 mg/kg, 0.92 ${\pm}$ 0.00 mg/kg and 1.08 ${\pm}$ 0.01 mg/kg, respectively. The lowest level of grayanotoxin III was 0.25 ${\pm}$ 0.01 mg/kg and the highest level was 3.29 ${\pm}$ 0.74 mg/kg. Through this study, safety management for foreign wild honey has been enabled.

• Journal of the Korean Chemical Society
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• v.57 no.1
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• pp.40-51
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• 2013

In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

• Journal of Forest and Environmental Science
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• v.38 no.3
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• pp.159-173
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• 2022

Genus of Rhododendron has been used in traditional medicine since ancient times and is known to be effective in immune function, inflammation, and cold symptoms. And the reason for this activity is the flavanonol type among flavonoids in the genus of Rhododendron. Among the flavanonol types, Taxifolin-3-O-arabinopyranoside was isolated from the root of native R. mucronulatum in Korea, and the structure was finally identified through HPLC, LC-MS/MS, ¹H-NMR, and ¹³C-NMR. Taxifolin-3-O-arabinopyranoside is a compound mainly found in R. mucronulatum, a representative species of the genus of Rhododendron, and exhibits antioxidant, anti-inflammatory, and anti-atopic activities. In this study, Taxifolin-3-O-arabinopyranoside was chemotaxonomic significant in 5 species of the genus Rhododendron native to Korea (R. mucronulatum, R. mucronulatum var. ciliatum, R. schlippenbachii, R. yedoense var. Poukhanense, R. japonicum for. Flavum). Compared with the existing literature, Taxifolin-3-O-arabinopyranoside was identified for the first time in 4 species of Rhododendron except for the R. mucronulatum.

• Journal of the Korean Wood Science and Technology
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• v.41 no.6
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• pp.566-575
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• 2013

The fruits of Taxus cuspidata were collected, divided into seeds and fruits, and extracted with 95% EtOH. The extracts were evaporated under the reduced vacuum pressure, concentrated, then successively fractionated with a series of n-hexane, dichloromethane, ethyl acetate and water on a separatory funnel to get some freeze dried samples. A portion of the EtOAc (arils:1.65 g, seeds:1.04 g) and $H_2O$ (arils:7 g, seeds:10 g) soluble samples were chromatographed on a Sephadex column using MeOH-$H_2O$ (1:1, 1:3, 1:5, v/v), EtOH-hexane (3:1, v/v) mixture and 100% $H_2O$ as eluting solvents to isolate pure compounds from the fractions. The isolates were developed by cellulose TLC using t-BuOH-HOAc-$H_2O$ (TBA; 3:1:1, v/v/v) and 6% aqueous HOAc. Visualization was done under ultraviolet light and by spraying the vanillin-HCl-EtOH reagent (4.8:12:480, v/v/v). followed by heating. The structures of the isolates were characterized by $^1H$- and $^{13}C$-NMR, DEPT, 2D-NMR, LC/MS and EI-MS spectra. In addition to the NMR and MS spectra, acid hydrolysis and permethylation were used to determine the correct structure of the isolated sugar compound. Their structures were elucidated as (+)-catechin (1), (-)-epicatechin (2), (+)-gallocatechin (3), (-)-epigallocatechin (4) and ${\beta}$-D-fructofuranose-($2{\rightarrow}4$)-O-${\beta}$-D-glucopyranose($1{\rightarrow}4$)-O-${\alpha}$-D-glucopyranose ($1{\rightarrow}2$)-O-${\beta}$-D-fructofuranose (5) on the basis of the above experimental evidences.

• Bulletin of the Korean Chemical Society
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• v.32 no.1
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• pp.109-112
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• 2011

A new derivative of tacrolimus was evaluated for its molecular weight, using LC-MS of the tacrolimus bulk active pharmaceutical ingredient (API) recovered through the purification of crude tacrolimus produced by Streptomyces clavuligerus CKD-1119. In addition, the molecular weight of the new derivative of tacrolimus was found to be at m/z 818 and was identified by $^{13}C$-NMR with peak assignments based on the differences in methyl group location resulting from the chemical structure. The structure of the new derivative, an unknown impurity of tacrolimus, was found to be 18-methyltacrolimus through comparison of the spectral data of the structural differences between ascomycin, tacrolimus, and the new derivative 18-methyltacrolimus.

• Natural Product Sciences
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• v.21 no.3
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• pp.162-169
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• 2015

Hamamelis japonica (Hamamelidaceae), widely known as Japanese witch hazel, is a deciduous flowering shrub that produces compact clumps of yellow or orange-red flowers with long and thin petals. As a part of our ongoing search for phenolic constituents from this plant, eleven phenolic constituents including six flavonol glycosides, a chalcone glycoside, two coumaroyl flavonol glycosides and two galloylated compounds were isolated from the flowers. Their structures were elucidated as methyl gallate (1), myricitrin (2), hyperoside (3), isoquercitrin (4), quercitrin (5), spiraeoside (6), kaempferol 4'-O-β-glucopyranoside (7), chalcononaringenin 2'-O-β-glucopyranoside (8), trans-tiliroside (9), cis-tiliroside (10), and pentagalloyl-O-β-D-glucose (11), respectively. These structures of the compounds were identified on the basis of spectroscopic studies including the on-line LCNMR-MS and conventional NMR techniques. Particularly, directly coupled LC-NMR-MS afforded sufficient structural information rapidly to identify three flavonol glycosides (2 - 4) with the same molecular weight in an extract of Hamamelis japonica flowers without laborious fractionation and purification step. Cytotoxic effects of all the isolated phenolic compounds were evaluated on HCT116 human colon cancer cells, and pentagalloyl-O-β-D-glucose (11) was found to be significantly potent in inhibiting cancer cell growth.

• Journal of the Korean Chemical Society
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• v.54 no.4
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• pp.443-446
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• 2010

HPLC analysis of a commercial herb drink marketed as a functional food revealed to contain an unauthorized substance similar to sildenafil, the active ingredient of the prescription drug Viagra$^{(R)}$ approved for the treatment of male erectile dysfunction. In order to identify the illegal additive, the herb drink was extracted with methylene chloride, and the extract was purified further using semipreparative HPLC. The chemical structure of the isolated substance was elucidated based on IR, LC/MS-ESI, and NMR spectroscopy, which showed the characteristics similar to sildenafil with minor modification. The only difference was the substitution of the methylpiperazine moiety of sildenafil to the hydroxyethylpiperazine group of the illegal additive.

• KSBB Journal
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• v.23 no.2
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• pp.153-157
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• 2008

Maca (Lepidium meyenii) has been used as a food and medicine in Peru for thousands of years. More recently a wide array of commercial maca products have gained popularity as dietary supplements with claims of anabolic and aphrodisiac effects. Even though the biologically active principles of maca are not fully known, the lipidic extract of maca tubers containing macamides showed promising physiological activities. In this study, the lipidic extract were collected from maca tubers by using supercritical carbon dioxide ($SCO_2$). Substance estimated as macamide in the extract was isolated and purified by preparative HPLC with recycling system. Two of the purified substance was identified as N-benzyl-5-oxo-6E,8E-octadecadienamide and N-benzylhexadecan amide by LC/MS, $^1H$-NMR and $^{13}C$-NMR analyses.

• Advances in nano research
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• v.10 no.5
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• pp.461-470
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• 2021

Infection is one of the major mortality causes throughout the globe. Nuclear medicine plays an important role in diagnosis of deep infections such as osteomyelitis, arthritis infection, heart valve and heart prosthesis infections. Techniques such as labeled leukocytes are sensitive and selective for tracking the inflammations but they are not suitable for differentiating infection from inflammation. Anionic linear-globular dendrimer-G₂ was synthesized then conjugation to gemifloxacin antibiotic. The structures were identified by FT-IR, ¹H-NMR, C-NMR, LC-MS and DLS. The toxicity of gemifloxacin and dendrimer-gemifloxacin complex was compared by MTT test. Dendrimer-G₂-gemifloxacin was labeled by Technetium-99m and its in-vitro stability and radiochemical purity were investigated. In-vivo biodistribution and SPECT imaging were studied in a rabbit model. Identify and verify the structure of the each object was confirmed by FT-IR, ¹H-NMR, C-NMR and LC-MS, also, the size and charge of this compound were 128 nm and -3/68 mv respectively. MTT test showed less toxicity of the dendrimer-G₂-gemifloxacin than free gemifluxacin (P < 0.001). Radiochemical yield was > %98. Human serum stability was 84% up to 24 h. Biodistribution study at 50 min, 24 and 48 h showed that the complex is significantly absorbed by the intestine and accumulation in the lungs and affects them, finally excreted through the kidneys, biodistribution results are consistent with results from full image means of SPECT/CT technique.

• Microbiology and Biotechnology Letters
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• v.24 no.5
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• pp.540-545
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• 1996

A facultative anaerobe Enterococcus faecium 19-46-4 was used to study the production of an antimicrobial substance in anaerobic conditions. Major part of the antibiotic activity was found in the culture filtrate of the bacterium. The active compound was extracted by an equal volume of iso-butanol and concentrated in vacuo (at 50$\circ$C) before purification by C-18 liguid column chromatography and HPLC. A chromatographically pure compound was obtained by two passages of HPLC columns, The compound appeared as a pale-yellow powder. The yield was about 2.5 mg 1$^{-1}$ culture filtrate. The compound was named as KIST 194. KIST 194 were identified as cholic acid (3$\alpha$, 7$\alpha$, 12$\alpha$-trihydroxy-5$\beta$-cholan 24-oic acid) based on its physico-chemical properties determined by UV, IR, $^{1}H-NMR, $^{13}$C-NMR, El-MS and LC-MS.